CN114937743B - Organic/inorganic perovskite solar cell based on formamidino and preparation method thereof - Google Patents

Organic/inorganic perovskite solar cell based on formamidino and preparation method thereof Download PDF

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CN114937743B
CN114937743B CN202210515626.0A CN202210515626A CN114937743B CN 114937743 B CN114937743 B CN 114937743B CN 202210515626 A CN202210515626 A CN 202210515626A CN 114937743 B CN114937743 B CN 114937743B
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solar cell
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lead
layer
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CN114937743A (en
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李亮
曹风人
张鹏
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Suzhou University
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/80—Constructional details
    • H10K30/81—Electrodes
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/40—Thermal treatment, e.g. annealing in the presence of a solvent vapour
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention relates to an organic/inorganic perovskite solar cell based on formamidino and a preparation method thereof. The organic conjugated polymer electrode comprises a conductive substrate, an electron transport layer, a lead-based perovskite film, an organic conjugated polymer layer and an electrode layer which are sequentially arranged. The preparation process comprises the following steps: depositing an electron transport layer on the surface of the conductive substrate; then preparing a high-quality perovskite layer by two-step reaction of the prepared mixed precursor of lead iodide and organic powder (lead bromide or methylamine lead bromide) and the mixed precursor of formamidine iodide and methylamine chloride solution; finally, preparing an organic conjugated polymer layer and an electrode layer above the perovskite layer in sequence. The preparation method disclosed by the invention is simple in process, greatly enhances the stability of the device by means of seed solution, is low in raw material cost and high in efficiency, is favorable for commercial mass production, and has great application value.

Description

Organic/inorganic perovskite solar cell based on formamidino and preparation method thereof
Technical Field
The invention belongs to the technical field of solar cells, and particularly relates to a preparation method of a high-quality stable halogen perovskite film, and a scheme for preparing a perovskite solar cell by using the same.
Background
In the twenty-first century, there has been an increasing demand for energy, and with the massive use of fossil energy, the energy crisis problem has become serious, and the environmental problem has also worsened. To solve this problem, the existing energy structure must be changed, and sustainable green energy is developed, where solar energy is the largest and most potential clean energy source. The current commercial solar cell is mainly a silicon solar cell, the preparation process of a monocrystalline silicon solar cell in a first generation solar cell is harsh, the cost is high, the process is complex, the cost of a polycrystalline silicon cell in a second generation solar cell is relatively advantageous, but the problems of defects and impurities are very large, so that the commercialization of a third generation thin film solar cell is very important, and the perovskite thin film solar cell has good prospect.
The perovskite thin film solar cell has the following main advantages compared with other solar cells: 1. the raw materials are low in cost; 2. the preparation process of the device is simple; 3. the photoelectric conversion efficiency is high, and the development speed is high. However, the main disadvantage of the perovskite solar cell is reflected in the long-term stability of the device, and the existing perovskite solar cell still far does not reach the commercial standard, so that the improvement of the stability of the perovskite solar cell is a popular research direction at present. In the literature reported previously, we can see that there are mainly several approaches to improve device performance and stability: 1. a blocking layer is added between the perovskite layer and the hole transmission layer, or a layer is added between the hole transmission layer and the metal electrode; 2. the intrinsic stability of the thin film is generally improved in a manner of doping new materials through optimizing the perovskite layer thin film; 3. the device is protected by a form of encapsulation of the polymer or other material. These approaches, of course, all serve to some extent to improve performance and stability, but are some distance from the commercial standards. Further invention and utilization of the novel approach to enhance perovskite stability is of great importance.
Disclosure of Invention
To solve the above mentioned stability problems. The invention provides a preparation method which is simple in preparation process and capable of effectively improving photoelectric conversion efficiency and stability of a battery.
The first object of the invention is to provide a perovskite solar cell with high performance and stability, which comprises a conductive substrate, an electron transport layer, a lead-based perovskite thin film, a p-type organic conjugated polymer layer and an electrode layer which are sequentially arranged.
In one embodiment of the invention, the lead-based perovskite thin film is prepared by the following method: and coating the perovskite precursor solution A on the electron transport layer, coating the perovskite precursor solution B, and annealing and crystallizing the film obtained by the reaction after the reaction is finished to obtain the lead-based perovskite film.
In one embodiment of the present invention, the perovskite precursor solution a is composed of lead iodide (PbI 2 ) And bromide; wherein the bromide is methylamine bromide (MABr) and/or methylamine lead bromide (MAPbBr) 3 )。
In one embodiment of the invention, the lead iodide concentration is 0.5-1.5 moles per liter, MABr or MAPbBr 3 The molar ratio of the lead iodide to the lead iodide is 0.1-10%.
In one embodiment of the present invention, the solvent of the perovskite precursor solution a is a mixed solvent of dimethyl sulfoxide (DMSO) and Dimethylformamide (DMF).
In one embodiment of the invention, the perovskite precursor solution B is obtained by mixing formamidine iodide (FAI) and methylamine chloride (MACl); wherein, the concentration of the formamidine iodide is 70-110 milligrams per milliliter, and the concentration of the methylamine chloride is 0-15 milligrams per milliliter; the solvent is isopropyl alcohol (IPA) solution.
In one embodiment of the invention, the electron transport layer has a thickness of 10-200 nanometers.
In one embodiment of the present invention, the electron transport layer is made of n-type metal oxide; the n-type metal oxide is selected from one or more of tin oxide, titanium oxide, niobium oxide and zinc oxide.
In one embodiment of the invention, the hole transport layer has a thickness of 10-300 nanometers.
In one embodiment of the present invention, the p-type organic conjugated polymer in the p-type organic conjugated polymer layer is selected from the group consisting of tetrakis [ N, N-bis (4-methoxyphenyl) amino groups]Spirobifluorene (Spiro-OMeTAD), poly (3-hexylthiophene-2, 5-diyl) (P 3 HT) and polythiophene-pyrrolopyrroldiketone (PDPP) 3 T) one or more of the following.
In one embodiment of the invention, the electrode layer material is a conductive metallic material and/or a carbon material.
The second object of the present invention is to provide a method for manufacturing the perovskite solar cell, comprising the steps of:
(1) Preparing an electron transport layer on a conductive substrate (ITO) and annealing in air at 100-150 ℃ for 5-60 minutes;
(2) Coating perovskite precursor solution A on the electron transport layer in the step (1), then dynamically coating perovskite precursor solution B, reacting, and annealing and crystallizing the film obtained by the reaction at 100-150 ℃ for 5-20 minutes to obtain the lead-based perovskite film;
(3) And (3) preparing a hole transport layer and an electrode on the lead-based perovskite film prepared in the step (2).
In one embodiment of the invention, in step (2), the reaction time is 10-60 seconds.
In one embodiment of the invention, in step (2), the annealing temperature is 100-150 ℃ and the time is 5-20 minutes.
In one embodiment of the present invention, in step (3), the steps of: the p-type organic conjugated polymer is deposited on the lead-based perovskite thin film, followed by deposition of a metal electrode or a carbon electrode.
In one embodiment of the present invention, the step (1) specifically includes the steps of: a metal oxide dispersion of a certain concentration (solubility of 1-10%) is prepared and then deposited on the cleaned transparent conductive substrate. Preferably, the preparation method is spin coating, the rotation speed and time are adjusted to 2000-5000 rpm and 20-50 seconds respectively, the freshly prepared metal oxide dispersion is dripped on the cleaned transparent conductive substrate, a spin coater is started after the dispersion is uniform, and then the chip with the spin tin oxide is placed on a hot table at 100-150 ℃ for annealing for 5-60 minutes.
In one embodiment of the invention, step (2) comprises the steps of: the lead iodide, MABr or MAPbBr with a certain proportion 3 The mixed solution is used as perovskite precursor solution A, pbI 2 At a concentration of 0.5-1.5 mol/liter MABr or MAPbBr 3 The molar ratio of the lead iodide to the lead iodide is 0-10%. The solvent is a mixed solution of dimethyl sulfoxide and dimethylformamide, wherein the proportion of the dimethyl sulfoxide is 0-100%. Mixing FAI and MACl solution at a certain ratio as precursor solution B, wherein FAI concentration is 70-110 mg/ml, and MACl concentration is 0-15 mlGrams per milliliter, the solvent was an isopropyl alcohol solution. Preferably, the preparation method is spin coating, spin coating parameters are well adjusted, namely the rotation speed is 2000-4000 rpm, the acceleration is 500-2000 rpm/s, the spin coating time is 30 seconds, precursor solutions of lead iodide and organic powder are firstly dripped, FAI and MACl precursor solutions are dynamically added in the spin coating process, and then the prepared film is annealed on a hot table at 100-150 ℃ for 5-20 minutes.
In one embodiment of the invention, step (3) comprises the steps of: a concentration of p-type organic conjugated polymer is formulated and then deposited on the prepared perovskite film. Then a layer of metal electrode or carbon electrode is deposited. Preferably, the p-type organic conjugated polymer is a Spiro-OMeTAD, 50-100 mg of Spiro-OMeTAD is dissolved in 1 ml of chlorobenzene solution, 10-50. Mu.l of tetra-t-butylpyridine (TBP) is added and stirred for 5-20 minutes, and 10-50. Mu.l of lithium bis (trifluoromethane) sulfonate (Li-TFSI) (260 mg of Li-TFSI in 1 ml of acetone) is added and stirred for 2-4 hours. After filtration, the formulated Spiro-OMeTAD solution was deposited on the cooled perovskite film. Finally oxidizing in oxygen for 8-16 hours.
In one embodiment of the invention, the electrode material of the electrode layer is silver (50-200 nm) and the preparation method is a thermal evaporation method.
Compared with the prior art, the technical scheme of the invention has the following advantages:
the invention simplifies the flow of the normal static two-step method, so that the preparation of the film is simpler; the existence of the second seed solution can improve the film forming quality of the film, so that the performance of the device is improved, and the highest photoelectric conversion efficiency can reach 23.22%; the presence of the third seed solution induces the formation of a more robust perovskite film, resulting in a more stable battery device that retains initial efficiency after 900 hours in the long-term stability test. This is mainly because, in order to stabilize the structure of the perovskite thin film, it is generally necessary to introduce a small amount of bromide ions, but the component formed with bromide ions having smaller ionic radii tends to have a stronger molecular polarity and thus is more susceptible to attack by moisture in the air. The seed solution method can enable Br ions gathered on the surface of the traditional two-step method to move downwards into the film, so that the damage to devices caused by water erosion is reduced. Compared with the traditional two-step method, the perovskite thin film has larger crystal grains and fewer defects, effectively improves the performance and stability of the device, has low cost of raw materials required by the method, has relatively simple preparation process, is beneficial to large-scale production in commercialization, and has great utilization value.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings, in which
FIG. 1 is a Scanning Electron Microscope (SEM) image of a perovskite thin film prepared according to example 1 of the invention;
fig. 2 is a graph showing current-voltage characteristics in examples of the present invention and comparative examples;
fig. 3 is a graph showing the long-range stability of the devices in examples and comparative examples of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
The invention provides a preparation technology of a perovskite solar cell with high efficiency and stability, which is characterized in that an organic powder material is added into a lead iodide precursor solution in a two-step method, and then a dynamic two-step method is used. The method comprises the steps of preparing an electron transport layer on conductive glass by a spin coating method, improving the crystallinity of a film by an annealing process, preparing a perovskite light absorption layer by a dynamic two-step method by using a treated precursor solution, and finally preparing a hole transport layer and an electrode layer to obtain the solar cell device.
Example 1:
the conductive substrate ITO is respectively soaked in acetone, alcohol and deionized water for ultrasonic cleaning for 20 minutes, and then is placed in an ultraviolet ozone cleaning machine for further treatment for 20 minutes. Commercial tin dioxide is then purchased(15% strength) with water at 1: 3. 70 microliters of just prepared tin oxide solution is dripped on a cleaned ITO chip by using a liquid-transferring gun, a spin coater is started after the solution is smeared uniformly, the rotation speed and the time are respectively adjusted to 4000r/s and 30s, and then the chip after the spin-coating of the tin oxide is placed on a hot table at 150 ℃ for annealing for 20 minutes. And after the annealing is finished, putting the flakes into an ultraviolet ozone cleaning machine for processing for 10 minutes. As for the perovskite layer, a bottle of 693 mg of PbI was prepared 2 And 10 mg of MABr in 900. Mu.l DMF and 100. Mu.l DMSO, and then a bottle of solution containing 90 mg of FAI and 9 mg of MACl in 1 ml of isopropanol was prepared. The spin parameters were then adjusted to a spin speed of 2000 rpm, an acceleration of 1000 rpm/sec, a spin time of 30 seconds, a first step of dispensing 50 μl of precursor solutions of lead iodide and organic powder, and a dynamic dispensing of 50 μl of precursor solutions of FAI and MACl when the spin time remained for only 16 seconds, followed by annealing the prepared film on a hot stage at 150 ℃ for 10 minutes. For the hole transport layer, 72.3 mg of Spiro-OMeTAD was first dissolved in 1 ml of chlorobenzene solution, followed by stirring on a cold table for one hour, then 35. Mu.l of TBP was added and stirred for half an hour, finally 35. Mu.l of Li-TFSI (260 mg of Li-TFSI in 1 ml of acetone) was added and stirred for two hours. And after the annealing of the perovskite film is completed and the perovskite film is cooled to room temperature, taking 20 microliters of prepared Spiro-OMeTAD solution to spin-coat the surface of the perovskite film, wherein spin-coating parameters are consistent with those of the perovskite layer. And finally, placing the prepared flakes in a vacuum cabin for oxygenizing for 12 hours by oxygen, then placing the flakes in a template, and evaporating a layer of silver with the thickness of 90 nanometers by a thermal evaporation instrument. The grain size of the thin film of the perovskite solar cell prepared by the method can reach 1.9 microns, the photoelectric conversion efficiency is 23.22%, and the device performance is not attenuated compared with the initial performance in 900 hours in the atmosphere with the humidity of about 40%.
Embodiment two:
a perovskite solar cell was prepared according to the procedure in example 1, except that the MABr mass in the procedure was changed to 50 mg. The performance of the composite photovoltaic cell prepared was slightly lower than in example 1.
Implementation scheme III:
perovskite solar cells were prepared according to the procedure in example 1, except that MABr in the procedure was changed to MAPbBr 3 . The performance of the composite photovoltaic cell prepared was slightly lower than in example 1.
Comparative example one:
perovskite solar cell was prepared according to the procedure in example one, except that in PbI 2 MABr is not added to the solution, i.e., no seed layer solution is built. The final photoelectric conversion efficiency can only reach 21.69%, and the device performance is attenuated by more than 60% compared with the initial performance after 900 hours in the atmosphere with the humidity of about 40%.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.

Claims (9)

1. An organic/inorganic perovskite solar cell based on formamidino, which is characterized in that: the organic light-emitting diode comprises a conductive substrate, an electron transport layer, a lead-based perovskite film, a p-type organic conjugated polymer layer and an electrode layer which are sequentially arranged; coating perovskite precursor solution A on the electron transport layer, coating perovskite precursor solution B, and annealing and crystallizing the film obtained by the reaction after the reaction is finished to obtain the lead-based perovskite film; the perovskite precursor solution A is obtained by mixing lead iodide and bromide; the perovskite precursor solution B is obtained by mixing formamidine iodide and methylamine chloride.
2. Formamidino-based organic/inorganic perovskite solar cell according to claim 1, characterized in that the bromide is methylamine bromine and/or methylamine lead bromine.
3. The formamidino-based organic/inorganic perovskite solar cell according to claim 1, wherein the concentration of lead iodide is 0.5-1.5 mol/l and the molar ratio of bromide to lead iodide is 0.1-10%.
4. The formamidine-based organic/inorganic perovskite solar cell according to claim 1, wherein the concentration of formamidine iodide is 70-110 mg/ml and the concentration of methylamine chloride is 0-15 mg/ml.
5. The formamidine-based organic/inorganic perovskite solar cell according to claim 1, wherein the thickness of the electron transport layer is 10-200 nanometers.
6. The formamidino-based organic/inorganic perovskite solar cell according to claim 1, wherein the electron transport layer is made of n-type metal oxide; the n-type metal oxide is selected from one or more of tin oxide, titanium oxide, niobium oxide and zinc oxide.
7. The formamidino-based organic/inorganic perovskite solar cell according to claim 1, wherein the p-type organic conjugated polymer in the p-type organic conjugated polymer layer is selected from one or more of tetrakis [ N, N-bis (4-methoxyphenyl) amino ] spirobifluorene, poly (3-hexylthiophene-2, 5-diyl) and polythiophene-pyrrolopyrroldiketone.
8. The formamidine-based organic/inorganic perovskite solar cell according to claim 1, wherein the electrode layer material is a conductive metal material and/or carbon material.
9. The method for producing a formamidino-based organic/inorganic perovskite solar cell according to any one of claims 1 to 8, comprising the steps of:
(1) Preparing an electron transport layer on a conductive substrate, and annealing at 100-150 ℃ in air for 5-60 minutes;
(2) Coating perovskite precursor solution A on the electron transport layer in the step (1), then dynamically coating perovskite precursor solution B, reacting, and annealing and crystallizing the film obtained by the reaction at 100-150 ℃ for 5-20 minutes to obtain the lead-based perovskite film;
(3) And (3) preparing a hole transport layer and an electrode on the lead-based perovskite film prepared in the step (2).
CN202210515626.0A 2022-05-12 2022-05-12 Organic/inorganic perovskite solar cell based on formamidino and preparation method thereof Active CN114937743B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106558650A (en) * 2016-12-07 2017-04-05 北京科技大学 A kind of preparation method of flexible copper indium gallium selenide/perovskite lamination solar cell
CN110246967A (en) * 2019-05-08 2019-09-17 电子科技大学 A kind of method of low temperature preparation flexibility perovskite solar battery
CN111640871A (en) * 2020-06-16 2020-09-08 西南石油大学 Perovskite solar cell capable of inhibiting photodecomposition of passivation layer and preparation method
CN113659082A (en) * 2021-08-17 2021-11-16 江苏盛开高新材料有限公司 Interface modification-based perovskite solar cell preparation method
CN113921720A (en) * 2021-10-12 2022-01-11 华能新能源股份有限公司 Treatment method of metal oxide-perovskite interface and battery

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106558650A (en) * 2016-12-07 2017-04-05 北京科技大学 A kind of preparation method of flexible copper indium gallium selenide/perovskite lamination solar cell
CN110246967A (en) * 2019-05-08 2019-09-17 电子科技大学 A kind of method of low temperature preparation flexibility perovskite solar battery
CN111640871A (en) * 2020-06-16 2020-09-08 西南石油大学 Perovskite solar cell capable of inhibiting photodecomposition of passivation layer and preparation method
CN113659082A (en) * 2021-08-17 2021-11-16 江苏盛开高新材料有限公司 Interface modification-based perovskite solar cell preparation method
CN113921720A (en) * 2021-10-12 2022-01-11 华能新能源股份有限公司 Treatment method of metal oxide-perovskite interface and battery

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